CN116497231B - Method for preparing nickel from tetra (trifluorophosphine) nickel - Google Patents
Method for preparing nickel from tetra (trifluorophosphine) nickel Download PDFInfo
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- CN116497231B CN116497231B CN202310738076.3A CN202310738076A CN116497231B CN 116497231 B CN116497231 B CN 116497231B CN 202310738076 A CN202310738076 A CN 202310738076A CN 116497231 B CN116497231 B CN 116497231B
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- trifluorophosphine
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- ammonia water
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 101
- -1 tetra (trifluorophosphine) nickel Chemical compound 0.000 title claims abstract description 62
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 36
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 44
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 44
- 239000007787 solid Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 238000005054 agglomeration Methods 0.000 claims abstract description 4
- 230000002776 aggregation Effects 0.000 claims abstract description 4
- 230000001737 promoting effect Effects 0.000 claims abstract description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 239000000047 product Substances 0.000 description 13
- 230000007062 hydrolysis Effects 0.000 description 12
- 238000006460 hydrolysis reaction Methods 0.000 description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- WKFBZNUBXWCCHG-UHFFFAOYSA-N phosphorus trifluoride Chemical compound FP(F)F WKFBZNUBXWCCHG-UHFFFAOYSA-N 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a method for preparing nickel by using tetra (trifluorophosphine) nickel, which comprises the following steps: step 1, dropwise adding ammonia water into tetra (trifluorophosphine) nickel liquid at a low temperature, stirring and hydrolyzing, and hydrolyzing the tetra (trifluorophosphine) nickel to generate nickel, phosphorous acid and hydrofluoric acid, wherein the phosphorous acid, the hydrofluoric acid and the ammonia water perform neutralization reaction to obtain suspension; step 2, heating the suspension obtained in the step 1 to enable ammonia which does not participate in the reaction to be discharged out of the system, simultaneously promoting agglomeration of small metal nickel particles to form larger particles to precipitate out of the solution, cooling and filtering to obtain a solid; and step 3, washing and drying the solid obtained in the step 2 to obtain nickel powder. The invention has mild condition, safe operation and high product purity.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a method for preparing nickel from tetra (trifluorophosphine) nickel.
Background
Nickel has 5 stable isotopes, and nickel materials are important in the fields of medicine, high-energy batteries and the like. For example, the nickel battery has the advantages of long service life, high energy density, strong environmental adaptability, easy integration, stable output and the like, is widely applied to the civil fields of medicine, micro-electric machinery, electronic products, electric automobiles and the like, and is a new energy battery with wide application prospect.
The excellent performance of nickel batteries determines great development potential, so that not only is the market demand urgent, but also the future will occupy an irreplaceable important place in the energy market. High-purity metallic nickel is an essential raw material for preparing a nickel battery, and in order to obtain the simple substance of nickel, one important reaction step is to prepare nickel by taking tetra (trifluorophosphine) nickel as a raw material.
The applicability of preparing nickel from tetra (trifluorophosphine) nickel as a raw material is concentrated in a specific field, and the method which can be found at present is only a thermal decomposition method. This process is a conventional process for preparing metallic nickel from tetrakis (trifluorophosphine) nickel, but has its drawbacks such as: the thermal decomposition process of the tetra (trifluorophosphine) nickel can generate gaseous phosphorus trifluoride in a reaction system, so that the pressure in a reaction container is increased, and the safety risk is caused; the generated phosphorus trifluoride gas is a severe poison and is easy to cause poisoning of operators and environmental pollution; the generated metallic nickel covers the inner wall of the reactor, and is difficult to take out and use.
The method for preparing high-purity nickel by using tetra (trifluorophosphine) nickel as a raw material adopts a neutralization method, and the current research is still in a blank stage.
Disclosure of Invention
The invention aims at overcoming the technical defects in the prior art and provides a method for preparing nickel by using tetra (trifluorophosphine) nickel.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a method for preparing nickel from tetra (trifluorophosphine) nickel, comprising the following steps:
step 1, dropwise adding ammonia water into tetra (trifluorophosphine) nickel liquid at the temperature of minus 20-0 ℃, stirring and hydrolyzing, and hydrolyzing the tetra (trifluorophosphine) nickel to generate nickel, phosphorous acid and hydrofluoric acid, wherein the phosphorous acid, the hydrofluoric acid and the ammonia water perform neutralization reaction to obtain a suspension;
step 2, heating the suspension obtained in the step 1 to enable ammonia which does not participate in the reaction to be discharged out of the system, simultaneously promoting agglomeration of small metal nickel particles to form particles to precipitate from the solution, cooling and filtering to obtain a solid;
and step 3, washing and drying the solid obtained in the step 2 to obtain nickel powder.
In the above technical scheme, in the step 1, when ammonia water is added dropwise, the temperature of the reaction system is controlled to be not higher than 5 ℃.
In the above technical scheme, in the step 1, the ammonia water is electronic grade ammonia water with a content of 25-28%, and a mass ratio of tetra (trifluorophosphine) nickel to electronic grade ammonia water is (30-40): (250-300).
In the above technical scheme, in the step 1, the ammonia water is completely dripped within 5-6.5 h, and stirring is continued for 0.5-1 h after the ammonia water dripping is completed.
In the above technical scheme, the step 1 uses alkali liquor to absorb tail gas.
In the above technical scheme, in the step 2, the heating temperature is 80-100 ℃ and the heating time is 4-5 h.
In the above technical solution, the tail gas is absorbed by water in the step 2.
In the above technical scheme, in the step 3, the washing is performed with ultrapure water and ammonia water under heating.
In the above technical solution, in the step 3, the washing includes the following steps:
step s1, adding the solid obtained in the step 2 into ultrapure water, and heating under the condition of stirring to ensure that the system is kept at the temperature of more than or equal to 80 ℃ for 1-2 hours; filtering out the solid when the temperature of the washing liquid is reduced to be less than or equal to 60 ℃;
step s2, adding the solid obtained in the step s1 into electronic grade ammonia water, and heating under the condition of stirring to keep the system at 50-60 ℃ for 1-2 hours; filtering out the solid after the temperature of the washing liquid is reduced to room temperature;
step s3, repeating the ammonia washing of step s2 at least once;
and step s4, repeating the water washing process of the step s1 until the pH value of the washing liquid is 7-10.
In the above technical scheme, in the step 3, drying is performed for 4-6 hours at 200-205 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for preparing the high-purity nickel powder by taking the tetra (trifluorophosphine) nickel as the raw material and adopting the hydrolysis neutralization method is provided aiming at the blank of the research of preparing the high-purity nickel powder by the current hydrolysis neutralization method so as to meet the requirements of civil fields such as medicine, electric automobiles and the like;
2. the hydrolysis neutralization method has mild reaction conditions, and can lead the tetra (trifluorophosphine) nickel to react with alkali liquor at low temperature, thereby realizing the conversion from the tetra (trifluorophosphine) nickel to the nickel simple substance. The reaction is carried out in the solution, acidic substances such as phosphorous acid, hydrofluoric acid and the like generated by the hydrolysis of the tetra (trifluorophosphine) nickel can be neutralized with weak alkaline ammonia water to form salt, so that the generation of serious poison phosphorus trifluoride is avoided, and the risks of personnel injury and environmental pollution are reduced. In addition, the hydrolysis neutralization reaction is a liquid reaction, the reaction is carried out under normal pressure, a pressure vessel is not needed in the process, and the operation is safer. Finally, the product metallic nickel generated by the reaction exists in the form of fine powder, and can be directly applied to subsequent reactions without treatment;
3. the process for preparing the high-purity nickel powder by taking the tetra (trifluorophosphine) nickel as the raw material can lead the yield of the nickel powder product to reach more than 70 percent, and the purity of the product is more than or equal to 99 percent and completely reaches the standard.
Drawings
FIG. 1 is a reaction scheme.
FIG. 2 is a diagram showing the connection of the hydrolysis neutralization reaction equipment between tetra (trifluorophosphine) nickel and ammonia water.
FIG. 3 is a diagram of a heating process plant connection.
FIG. 4 is a connection diagram of a washing process device.
FIG. 5 shows the results of the test of the product of example 2.
FIG. 6 shows the results of the test of the product of example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1, a method for preparing nickel from tetra (trifluorophosphine) nickel comprises the following steps:
step 1, hydrolysis neutralization reaction:
hydrolysis neutralization comprises two reaction processes, namely hydrolysis of tetra (trifluorophosphine) nickel; and (3) neutralizing the hydrolysis products of phosphorous acid, hydrofluoric acid and weak alkaline ammonia water. The specific reaction process is as follows:
Ni(PF 3 ) 4 +12H 2 O=Ni+4H 3 PO 3 +12HF
H 3 PO 3 +3 NH 3 .H 2 O = (NH 4 ) 3 PO 3 +3H 2 O
3HF+3 NH 3 .H 2 O=3NH 4 F+3H 2 O
the connection diagram of the reaction equipment is shown in FIG. 2.
The operation process is as follows:
a. the system is connected with a polytetrafluoroethylene reaction kettle, a mechanical stirrer, a constant pressure dropping funnel, a low temperature constant temperature tank, various pipelines and a tail gas absorption bottle according to the figure 2;
b. and (3) weighing 33.60 g-34.30 g of tetra (trifluorophosphine) nickel, adding the nickel into the polytetrafluoroethylene reaction kettle, starting stirring, and regulating the rotating speed to 400-450 rpm. 274.50 g-275.50 g of electronic grade ammonia water with the content of 25-28% is weighed and added into a constant pressure dropping funnel;
c. setting the temperature of a low-temperature constant-temperature tank to-20-0 ℃, starting cooling circulation to cool tetra (trifluorophosphine) nickel liquid, when detecting that the tetra (trifluorophosphine) nickel liquid reaches the set temperature by using a thermometer, starting a constant-pressure dropping funnel, dropping ammonia water into the tetra (trifluorophosphine) nickel, observing the temperature of a reaction system on line, and controlling the dropping speed to ensure that the temperature of the reaction system is increased to be less than or equal to 5 ℃, and the ammonia water is dropped out within 5-6.5 hours;
d. after the ammonia water is added, continuing stirring for 0.5-1 h;
step 2, heating and filtering:
and heating the suspension obtained after the reaction to discharge ammonia which does not participate in the reaction in the solution out of the system, and promoting the agglomeration of small metal nickel particles to form larger particles to separate out precipitates from the solution. The reaction equipment is shown in FIG. 3;
the operation process comprises the following steps:
the system is connected with pipelines, a temperature controller, a polytetrafluoroethylene reaction kettle, an electric heating sleeve and a tail gas absorption bottle according to figure 3. Controlling the temperature of the reaction liquid to be 80-100 ℃, heating the reaction liquid in the polytetrafluoroethylene reaction kettle for 4-5 hours by using an electric heating sleeve, cooling, and filtering out solids;
step 3, washing and drying:
washing the precipitated solid with ultrapure water and aqueous ammonia, respectively, under heating, several times, wherein the ultrapure water washing is used for removing (NH) 4 ) 3 PO 3 、NH 4 Soluble salt impurities such as F; ammonia water is used for dissolving and removing a small amount of Ni mixed in the solid 3 (PO 4 ) 2 The schematic of the poorly soluble salt is shown in fig. 4:
description of operation:
a. adding the solid into a polytetrafluoroethylene reaction kettle, adding 200-300 ml of ultrapure water, and heating under the condition of stirring to keep the system at the temperature of more than or equal to 80 ℃ for 1-2 hours; filtering out the solid when the temperature of the washing liquid is reduced to be less than or equal to 60 ℃;
b. adding the solid into a polytetrafluoroethylene reaction kettle, adding 100-150 ml of electronic grade ammonia water, and heating under the condition of stirring to keep the system at 50-60 ℃ for 1-2 hours; filtering out the solid after the temperature of the washing liquid is reduced to room temperature;
c. repeating the ammonia washing process once;
d. repeating the water washing process for 3-4 times until the pH value of the washing liquid is 7-10;
drying the solid:
and placing the filtered solid into a polytetrafluoroethylene tray, placing the tray into an air-blast drying box, and drying for 4-6 hours at 200-205 ℃ to obtain the solid nickel powder.
Example 2
On the basis of example 1, a method for preparing nickel from tetra (trifluorophosphine) nickel comprises the following steps:
step 1, hydrolysis neutralization reaction:
33.80 g of tetra (trifluorophosphine) nickel is weighed into a polytetrafluoroethylene reaction kettle, stirring is started, and the rotating speed is regulated to 450rpm. And weighing 274.72g of electronic grade ammonia water with the content of 25-28%, and adding into a constant pressure dropping funnel. Setting the temperature of the low-temperature constant-temperature tank to-15 ℃, starting a cooling circulation to cool the tetra (trifluorophosphine) nickel liquid, starting a funnel after a thermometer detects that the tetra (trifluorophosphine) nickel reaches the set temperature, dropwise adding ammonia water into the tetra (trifluorophosphine) nickel, dropwise adding the ammonia water for 5h and 10min, and continuously stirring for 0.5h;
step 2, heating and filtering:
heating the reaction liquid, controlling the temperature to be 98.5-99 ℃ and preserving the heat for 4.5 hours, cooling and filtering out solids;
step 3, washing and drying:
200ml of ultrapure water was added to the solid, and the system was kept at 80℃for 1.5 hours with stirring, and the solid was filtered off when the temperature of the washing solution was lowered to 57.3 ℃. 120ml of electronic grade ammonia water is added into the solid, and the solid is heated under the condition of stirring, so that the system is kept for 1h at 55 ℃; after the wash solution had cooled to room temperature, the solid was filtered off. The ammonia wash process was repeated once. The washing procedure was repeated 3 times and the final wash was tested to have a pH of 8.05. Drying at 205℃for 4.5h gave a nickel powder product weighing 3.78g in 77.9% yield.
Example 3
The difference between this example and example 2 is that the amounts of ammonia water and tetra (trifluorophosphine) nickel used as the reaction raw materials are different, the ratio of ammonia water to tetra (trifluorophosphine) nickel in example 3 is reduced, the ratio of 8.13:1 in example 2 is reduced to 8.07:1, and the appropriate amount of ammonia water is reduced, so that the possibility of nickel ions and ammonia water react to form nickel hydroxide solid is reduced, the impurity content in the product can be reduced, and the purity of the product is finally improved.
A method for preparing nickel from tetra (trifluorophosphine) nickel, comprising the following steps:
step 1, hydrolysis neutralization reaction:
34.08g of tetra (trifluorophosphine) nickel is weighed into a polytetrafluoroethylene reaction kettle, stirring is started, and the rotating speed is regulated to 450rpm. And weighing 275.03g of electronic grade ammonia water with the content of 25-28%, and adding into a constant pressure dropping funnel. Setting the temperature of the low-temperature constant-temperature tank to-10 ℃, starting a cooling circulation to cool the tetra (trifluorophosphine) nickel, starting a funnel after a thermometer detects that the tetra (trifluorophosphine) nickel reaches the set temperature, dropwise adding ammonia water into the tetra (trifluorophosphine) nickel, and continuing stirring for 1h after the ammonia water is completely dripped for 5.5 h;
step 2, heating and filtering:
heating the reaction liquid, controlling the temperature to be 99.5-100 ℃ and preserving heat for 5 hours, cooling and filtering out solids;
step 3, washing and drying:
260ml of ultra pure water was added to the solid, and the system was kept at 90℃for 2 hours with stirring, and the solid was filtered off when the temperature of the washing solution was lowered to 50.5 ℃. 150ml of electronic grade ammonia water is added into the solid, and the solid is heated under the condition of stirring, so that the system is kept at 59 ℃ for 1.5h; after the wash solution had cooled to room temperature, the solid was filtered off. The ammonia wash process was repeated once. The washing procedure was repeated 4 times and the final wash was tested to have a pH of 8.35. Drying at 200 ℃ for 5.5h, the weight of the nickel powder product is 3.69g, and the yield is 75.5%.
The yield of the nickel powder products of example 2 and example 3 can reach more than 70%, and the product detection results are shown in fig. 5 and 6.
16 impurities are less than 1%, the purity of nickel metal is more than or equal to 99%, and through XRD detection, the simple substance structure of nickel is in a cubic phase crystal form, and the quality of the simple substance of nickel completely reaches the standard.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method for preparing nickel from tetra (trifluorophosphine) nickel, comprising the steps of:
step 1, dropwise adding ammonia water into tetra (trifluorophosphine) nickel liquid at the temperature of minus 20-0 ℃, stirring and hydrolyzing, and hydrolyzing the tetra (trifluorophosphine) nickel to generate nickel, phosphorous acid and hydrofluoric acid, wherein the phosphorous acid, the hydrofluoric acid and the ammonia water perform neutralization reaction to obtain a suspension;
step 2, heating the suspension obtained in the step 1 to enable ammonia which does not participate in the reaction to be discharged out of the system, simultaneously promoting agglomeration of small metal nickel particles to form particles to precipitate from the solution, cooling and filtering to obtain a solid;
and step 3, washing and drying the solid obtained in the step 2 to obtain nickel powder.
2. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in step 1, the temperature of the reaction system is controlled to be not higher than 5 ℃ when ammonia water is added dropwise.
3. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in the step 1, the ammonia water is electronic grade ammonia water with a content of 25-28%, and a mass ratio of tetra (trifluorophosphine) nickel to electronic grade ammonia water is (30-40): (250-300).
4. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in the step 1, ammonia water is dripped within 5-6.5 h, and stirring is continued for 0.5-1 h after the dripping of ammonia water is completed.
5. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein the tail gas is absorbed by alkaline solution in step 1.
6. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in the step 2, the heating temperature is 80-100 ℃ and the heating time is 4-5 h.
7. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein the tail gas is absorbed by water in step 2.
8. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in step 3, the nickel is washed with ultra pure water and aqueous ammonia, respectively, under heating.
9. The method for preparing nickel from tetrakis (trifluorophosphine) nickel according to claim 8, wherein the washing in step 3 comprises the steps of:
step s1, adding the solid obtained in the step 2 into ultrapure water, and heating under the condition of stirring to ensure that the system is kept at the temperature of more than or equal to 80 ℃ for 1-2 hours; filtering out the solid when the temperature of the washing liquid is reduced to be less than or equal to 60 ℃;
step s2, adding the solid obtained in the step s1 into electronic grade ammonia water, and heating under the condition of stirring to keep the system at 50-60 ℃ for 1-2 hours; filtering out the solid after the temperature of the washing liquid is reduced to room temperature;
step s3, repeating the ammonia washing of step s2 at least once;
and step s4, repeating the water washing process of the step s1 until the pH value of the washing liquid is 7-10.
10. The method for preparing nickel from tetra (trifluorophosphine) nickel according to claim 1, wherein in the step 3, the nickel is dried at 200-205 ℃ for 4-6 hours.
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